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Martins J.,Instituto Dos Vinhos Do Douro e Do Porto | Martins J.,Polytechnic Institute of Porto | Esteves C.,Instituto Dos Vinhos Do Douro e Do Porto | Simoes T.,Instituto Dos Vinhos Do Douro e Do Porto | And 2 more authors.
Journal of Agricultural and Food Chemistry | Year: 2011

The present work describes a solid-phase microextraction (SPME) gas chromatography-tandem mass spectrometry (MS/MS) method to quantify 24 pesticides in fortified white wine and fortified red wine. In this study "fortified wine" refers to a wine in which fermentation is arrested before completion by alcohol distillate addition, allowing sugar and alcoholic contents to be higher (around 80-100 g/L total sugars and 19-22% alcohol strength (v/v)). The analytical method showed good linearity, presenting correlation coefficients (R2) ≥ 0.989 for all compounds. Limits of detection (LOD) and quantitation (LOQ) in the ranges of 0.05-72.35 and 0.16-219.23 μg/L, respectively, were obtained. LOQs are below the maximum residue levels (MRL) set by European Regulation for grapes. The proposed method was applied to 17 commercial fortified wines. The analyzed pesticides were not detected in the wines tested. © 2011 American Chemical Society. Source


Martins J.,Instituto Dos Vinhos Do Douro e Do Porto | Martins J.,Polytechnic Institute of Porto | Esteves C.,Instituto Dos Vinhos Do Douro e Do Porto | Limpo-Faria A.,Instituto Dos Vinhos Do Douro e Do Porto | And 5 more authors.
Analytical Letters | Year: 2011

A SPME-GC-MS/MS method for the determination of eight organophosphorus pesticides (azinphos-methyl, chlorpyriphos, chlorpyriphos-methyl, diazinon, fenitrothion, fenthion, malathion, and methidathion) in still and fortified wine was developed. The extraction procedure is simple, solvent free, and without any sample pretreatment. Limits of detection (LOD) and quantitation (LOQ) values in the range 0.1-14.3 μg/L and 0.2-43.3 μg/L, respectively, were obtained. The LOQ values are below the maximum residue levels (MRLs) established by European Regulation for grapes, with the exception of methidathion. Coefficients of correlation (R2) higher than 0.99 were obtained for the majority of the pesticides, in all different wines analyzed. © Taylor & Francis Group. Source


Martins J.,Instituto Dos Vinhos Do Douro e Do Porto | Martins J.,Polytechnic Institute of Porto | Esteves C.,Instituto Dos Vinhos Do Douro e Do Porto | Limpo-Faria A.,Instituto Dos Vinhos Do Douro e Do Porto | And 5 more authors.
Food Chemistry | Year: 2012

A multiresidue gas chromatographic method for the determination of six fungicides (captan, chlorthalonil, folpet, iprodione, procymidone and vinclozolin) and one acaricide (dicofol) in still and fortified wines was developed. Solid-phase microextraction (SPME) was chosen for the extraction of the compounds from the studied matrices and tandem mass spectrometry (MS/MS) detection was used. The extraction consists in a solvent free and automated procedure and the detection is highly sensitive and selective. Good linearity was obtained with correlation coefficients of regression (R 2) > 0.99 for all the compounds. Satisfactory results of repeatability and intermediate precision were obtained for most of the analytes (RSD ≤ 20%). Recoveries from spiked wine ranged from 80.1% to 112.0%. Limits of quantification (LOQs) were considerably below the proposed maximum residue limits (MRLs) for these compounds in grapes and below the suggested limits for wine (MRLs/10), with the exception of captan. © 2011 Elsevier Ltd. All rights reserved. Source

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